JP7179441B2 - 多層カーボンナノチューブの合成のための触媒、及びその触媒で合成された多層カーボンナノチューブ - Google Patents
多層カーボンナノチューブの合成のための触媒、及びその触媒で合成された多層カーボンナノチューブ Download PDFInfo
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- JP7179441B2 JP7179441B2 JP2016543626A JP2016543626A JP7179441B2 JP 7179441 B2 JP7179441 B2 JP 7179441B2 JP 2016543626 A JP2016543626 A JP 2016543626A JP 2016543626 A JP2016543626 A JP 2016543626A JP 7179441 B2 JP7179441 B2 JP 7179441B2
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- carbon nanotubes
- walled carbon
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- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 description 2
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 2
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- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 description 2
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- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 1
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- 229940067460 calcium acetate monohydrate Drugs 0.000 description 1
- 229940050560 calcium chloride anhydrous Drugs 0.000 description 1
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 description 1
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- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 description 1
- ISPYRSDWRDQNSW-UHFFFAOYSA-L manganese(II) sulfate monohydrate Chemical compound O.[Mn+2].[O-]S([O-])(=O)=O ISPYRSDWRDQNSW-UHFFFAOYSA-L 0.000 description 1
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Description
しかしながら、本発明が解決しようとする課題は、以上で言及した課題に制限されず、言及されていない他の課題は、以下の記載から当業者に明確に理解されることができる。
Vt/c=(Wt×γt)/(Wc×γc) (1)
(式(1)で、γt=1/ρt、γc=1/ρcであり、
Wtは、単位触媒(1g)で成長させることができるカーボンナノチューブの重量、
Wcは、単位触媒の重量で1gであり、
ρtは、カーボンナノチューブの見掛け密度、ρcは触媒の見掛け密度である)。
本発明のまた他の側面は、多層カーボンナノチューブを含むエネルギー貯蔵装置を提供する。
[化学式1]
[Fea、Cob、Cac、Nid、Moe][Mnw、Alx、Mgy、Siz]
(上記化学式1中、a、b、c、d、e、w、x、y、zは、各元素のモル分率を表し、
0≦a≦10、0≦b≦10、0≦c≦10、0≦d≦10、0≦e≦10、0≦w≦30、0≦x≦30、0≦y≦30、0≦z≦30で、2≦a+b+c+d+e+w+x+y+z≦l70、2≦a+b+c+d+e≦50、2≦w+x+y+z≦50である)
Vt/c=(Wt×γt)/(Wc×γc) (2)
(式(2)中、γt=1/ρt、γc=1/ρcであり、
Wtは、単位触媒(1g)で成長させることができるカーボンナノチューブの重量、
Wcは、単位触媒の重量で1gであり、
ρtはカーボンナノチューブの見掛け密度、ρcは触媒の見掛け密度である)。
本発明のまた他の側面は、板状触媒を含むカーボンナノチューブを提供する。板状触媒の場合、球状または針状の触媒に比べて表面積が広く、触媒の上下面でカーボンナノチューブが同時に成長することができるという利点がある。
本発明の板状触媒の各面は扁平または曲率を有する曲面の形態(曲がった形態)であることができるが、これに限定されるものではない。
本発明の製造方法による触媒を利用して合成された多層カーボンナノチューブは、単層カーボンナノチューブ(SWNT)に匹敵する直径を有し、層(wall)の数が3~10個と非常に均質な状態であり、比表面積が大きくて、非常に高い導電性を示す。
また、本発明の触媒を利用して成長させたカーボンナノチューブは、98%以上の純度を有して同じ量の触媒を利用して数倍以上多い量の多層カーボンナノチューブを合成することができる。
本発明の一側面は、下記式(1)で表される触媒lg当たり成長した多層カーボンナノチューブの体積を触媒1gの体積で割った値が30以上の多層カーボンナノチューブを提供する:
Vt/c=(Wt×γt)/(Wc×γc) (1)
(式(1)中、γt=1/ρt、γc=1/ρcであり、
Wtは、単位触媒(1g)で成長させることができるカーボンナノチューブの重量、
Wcは、単位触媒の重量で1gであり、
ρtは、カーボンナノチューブの見掛け密度、ρcは触媒の見掛け密度である)。
[化学式1]
[Fea、Cob、Cac、Nid、Moe][Mnw、Alx、Mgy、Siz]
(上記「化学式1中、a、b、c、d、e、w、x、y、zは、各元素のモル分率を表し、
0≦a≦10、0≦b≦10、0≦c≦10、0≦d≦10、0≦e≦10、0≦w≦30、0≦x≦30、0≦y≦30、0≦z≦30で、2≦a+b+c+d+e+w+x+y+z≦l70、2≦a+b+c+d+e≦50、2≦w+x+y+z≦50である)
Vt/c=(Wt×γt)/(Wc×γc) (2)
(式(2)中、γt=1/ρt、γc=1/ρcであり、
Wtは、単位触媒(1g)で成長させることができるカーボンナノチューブの重量、
Wcは、単位触媒の重量で1gであり、
ρtはカーボンナノチューブの見掛け密度、ρcは触媒の見掛け密度である)。
水100mlにAlとMgのモル数の和が16になるようにMg(NO3)2.6H2OとA1C13・6H2Oを投入して攪拌しながら、FeとCoのモル数の和が5になるようにFe(NO3)2・9H2OとCo(NO3)2・6H2Oを投入して攪拌した。その後、上記混合物を400~900℃の範囲で液滴噴霧しながら焼成させて触媒を得た。
実施例1に記載された方法と同じ製造方法を使用し、AlとMgのモル数の和を20に変化させて、金属触媒を製造した。
上記実施例1で得られた触媒を利用して炭素源ガスと不活性ガスで反応器の温度を400~1200℃に昇温させる気相蒸着法を通じてカーボンナノチューブを製造した。
上記実施例2で得られた触媒を利用して炭素源ガスと不活性ガスで反応器の温度を400~1200℃に昇温させる気相蒸着法を通じてカーボンナノチューブを製造した。
実施例1及び実施例2によって比表面積が極大化された微粒子の板状触媒が製造された。
BET(Brunauer Emmett Teller)比表面積の測定結果は142m2/gであり、触媒の見掛け密度は韓国産業標準(KS M ISO 1306)を準用した。
即ち、見掛け密度を測定するために、直径が100±10mmで、一定高さの垂直層に口がなく、完全に満たしたとき、1000cm3の容量を有するシリンダー型容器の辺縁より50mm以上高くないところで容器の中央部分から触媒を入れ、この時、容器の辺縁よりも高く円錐形を形成することができるように過量の触媒を使用した。定規またはへらを水平にして、容器の辺縁に直角に隙間なく接触した後、一度擦って表面を均一にして、触媒と一緒に重量を測定した。シリンダーの重量を引いて最も近いg数に触媒の質量を決定した。
上記実施例1及び実施例2によって製造された触媒を利用して製造例1と製造例2の多層カーボンナノチューブを製造し、この時、触媒1g当たり合成されたカーボンナノチューブの量は、それぞれ90g及び80gであった。
製造例1と製造例2で合成された多層カーボンナノチューブの見掛け密度(KS M ISO 1306に基づいて測定)は、0.01g/mlであり、透過電子顕微鏡で測定したカーボンナノチューブの直径は5-8nmであった。
即ち、純度を測定するためにるつぼを密閉された電気炉で1時間550±25℃の温度で蓋をして加熱した後、るつぼと蓋をデシケーターに入れた。室温に冷却させ、0.1mgまで重量を測定した。2gが若干超えるカーボンナノチューブを125℃の乾燥機で1時間乾燥した後、室温に冷却させた。カーボンナノチューブを重量を測定したるつぼに入れて0.1mgまで重量を測定し、これを一定量になるまで800±25℃の電気炉の中に入れてふたを開けて加熱した。蓋を閉じ、デシケーターに移して室温に冷却させた後、0.1mgまで重量を測定した。るつぼと蓋を洗浄し、125℃の乾燥機の中で乾燥した後、0.1mgまで重量を再測定した。
即ち、単位触媒1gの体積は20mlであるので、板状触媒を利用して成長させた多層カーボンナノチューブの体積は9000ml(9Liter)であることを意味する。
図4に示すように、0.5重量%の多層カーボンナノチューブ(MWNT)の含有量から複合体は導電性を表し始め、多層カーボンナノチューブの含有量が増加するにつれて、複合体の導電性が急激に高くなることが分かる(多層カーボンナノチューブの含有量が増加するにつれて、表面抵抗の急速な減少が現れる)。
本発明の触媒を利用して合成した分散性が高い多層カーボンナノチューブは、低含量(0.5重量%)でもポリマーマトリックス内で高い導電性を表した。
多層カーボンナノチューブの合成のための触媒の製造方法を示す概略図は図5に示した。
また、本発明の製造方法で製造された触媒を利用して合成された高純度の多層カーボンナノチューブは、単層カーボンナノチューブ(SWNT)に匹敵する直径を有し、層の数が3~10個と非常に均質な状態であり、表面積が大きくて、非常に高い導電性を表している。
本発明の範囲は、上述した詳細な説明ではなく、後述する特許請求の範囲によって定められ、特許請求の範囲の意味及び範囲、そしてその均等な概念から導出されるすべての変更または変形された形態が本発明の範囲に含まれるものと解釈すべきである。
Claims (5)
- 下記式(1)で表される触媒1g当たり成長したカーボンナノチューブの体積を触媒1gの体積で割った値が120以上であり、表面積が600~1000m2/gであり、直径が3~10nmであり、層の数が3~6個であり、純度が98%以上である多層カーボンナノチューブ:
Vt/c=(Wt×γt)/(Wc×γc) (1)
(式(1)中、γt=1/ρt、γc=1/ρcであり、
Wtは、単位触媒(lg)で成長させることができるカーボンナノチューブの重量、
Wcは、単位触媒の重量で1gであり、
ρtは、カーボンナノチューブの見掛け密度、ρcは触媒の見掛け密度である)。 - 前記式(1)で表される触媒1g当たり成長したカーボンナノチューブの体積を触媒1gの体積で割った値が160以上である請求項1に記載の多層カーボンナノチューブ。
- 請求項1または2に記載の多層カーボンナノチューブを含む複合体。
- 請求項1または2に記載の多層カーボンナノチューブを含むエネルギー貯蔵装置。
- 下記式(1)で表される触媒1g当たり成長したカーボンナノチューブの体積を触媒1gの体積で割った値が120以上であり、表面積が600~1000m2/gであり、直径が3~10nmであり、層の数が3~6個である多層カーボンナノチューブ:
Vt/c=(Wt×γt)/(Wc×γc) (1)
(式(1)中、γt=1/ρt、γc=1/ρcであり、
Wtは、単位触媒(lg)で成長させることができるカーボンナノチューブの重量、
Wcは、単位触媒の重量で1gであり、
ρtは、カーボンナノチューブの見掛け密度、ρcは触媒の見掛け密度である)。
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PCT/KR2015/000053 WO2015105302A1 (ko) | 2014-01-09 | 2015-01-05 | 다중벽 탄소나노튜브 합성을 위한 촉매, 그 촉매의 제조 방법 및 그 촉매로 합성된 다중벽 탄소나노튜브 |
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